A buckminsterfullerene (C60)-based primary ion beam system has been developed for routine application in TOF-SIMS analysis of organic materials. The ion beam system is described, and its performance is characterized. Nanoamp beam currents of C60+ are obtainable in continuous current mode. C60(2+) can be obtained in pulsed mode. At 10 keV, the beam can be focused to less than 3 microm with 0.1 nA currents. TOF-SIMS studies of a series of molecular solids and a number of polymer systems in monolayer and thick film forms are reported. Very significant enhancement of secondary ion yields, particularly at higher mass, were observed using 10-keV C60+ for all samples other than PTFE, as compared to those observed from 10 keV Ga+ primary ions. Three materials (PS2000, Irganox 1010, PET) were studied in detail to investigate primary ion-induced disappearance (damage) cross sections to determine the increase in secondary ion formation efficiency. The C60 disappearance cross sections observed from monolayer film PS2000 and self-supporting PET film are close to those observed from Ga+. The resulting C60 efficiencies are 30-100 times those observed from gallium. The cross sections observed from C60 bombardment of multilayer molecular solids are approximately 100 times less, such that essentially zero damage sputtering is possible. The resulting efficiencies are > 10(3) greater than from gallium. It is also shown that C60 primary ions do not generate any more low-mass fragments than any other ion beam system does. C60 is shown to be a very favorable ion beam system for TOF-SIMS, delivering high yield, close to 10% total yield, favoring high-mass ions, and on thick samples, offering the possibility of analysis well beyond the static limit.
Time-of-flight secondary ion mass spectrometry (TOF-SIMS) has unique capabilities in the area of high-resolution mass spectrometric imaging of biological samples. The technique offers parallel detection of native and non-native molecules at physiological concentrations with potentially submicrometer spatial resolution. Recent advances in SIMS technology have been focused on generating new ion sources that can in turn be used to eject more intact molecular and biological characteristic species from a sample. The introduction of polyatomic ion beams, particularly C60, for TOF-SIMS analysis has created a whole new application of molecular depth profiling and 3D molecular imaging. However, such analyses, particularly at high lateral resolution, are severely hampered by the accompanying mass spectrometry associated with current TOF-SIMS instruments. Hence, we have developed an instrument that overcomes many of the drawbacks of current TOF-SIMS spectrometers by removing the need to pulse the primary ion beam. The instrument samples the secondary ions using a buncher that feeds into a specially designed time-of-flight analyzer. We have validated this new instrumental concept by analyzing a number of biological samples generating 2D and 3D images showing molecular localization on a subcellular scale, over a practical time frame, while maintaining high mass resolution. We also demonstrate large area mapping and the MS/MS capability of the instrument.
A chemical imaging time-of-flight secondary ion mass spectrometer is described. It consists of a liquid metal ion gun, medium energy resolution reflectron mass analyzer, liquid nitrogen cooled sample stage, preparation chamber and dual stage entry port. Unique features include compatibility with laser postionization experiments, large field of view, cryogenic sample handling capability and high incident ion beam current. Instrument performance is illustrated by the characterization of scanning electron microscopy grids, silver and functionalized polystyrene beads and the postionization of an organic overlayer on a gold substrate.
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